CN116904152A - Environment-friendly joint beautifying composition for ceramic tiles and preparation method thereof - Google Patents
Environment-friendly joint beautifying composition for ceramic tiles and preparation method thereof Download PDFInfo
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- CN116904152A CN116904152A CN202310513706.7A CN202310513706A CN116904152A CN 116904152 A CN116904152 A CN 116904152A CN 202310513706 A CN202310513706 A CN 202310513706A CN 116904152 A CN116904152 A CN 116904152A
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- 239000000203 mixture Substances 0.000 title claims abstract description 41
- 239000000919 ceramic Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 37
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 51
- 239000003607 modifier Substances 0.000 claims abstract description 35
- 239000011858 nanopowder Substances 0.000 claims abstract description 34
- 150000001412 amines Chemical class 0.000 claims abstract description 31
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 22
- 239000003822 epoxy resin Substances 0.000 claims abstract description 21
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 21
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 15
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 13
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 13
- 239000003085 diluting agent Substances 0.000 claims abstract description 11
- 239000003999 initiator Substances 0.000 claims abstract description 10
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 10
- 230000007613 environmental effect Effects 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 62
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 62
- 229910021389 graphene Inorganic materials 0.000 claims description 61
- 239000004005 microsphere Substances 0.000 claims description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 55
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 54
- 238000002156 mixing Methods 0.000 claims description 50
- 238000003756 stirring Methods 0.000 claims description 47
- 238000010438 heat treatment Methods 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 29
- 238000005406 washing Methods 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 23
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical group OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 21
- 239000005543 nano-size silicon particle Substances 0.000 claims description 20
- 238000001694 spray drying Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000013530 defoamer Substances 0.000 claims description 15
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000010276 construction Methods 0.000 claims description 12
- -1 alkyl orthosilicate Chemical compound 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 9
- 230000001804 emulsifying effect Effects 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- NPBVQXIMTZKSBA-UHFFFAOYSA-N Chavibetol Natural products COC1=CC=C(CC=C)C=C1O NPBVQXIMTZKSBA-UHFFFAOYSA-N 0.000 claims description 7
- 239000005770 Eugenol Substances 0.000 claims description 7
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 7
- UVMRYBDEERADNV-UHFFFAOYSA-N Pseudoeugenol Natural products COC1=CC(C(C)=C)=CC=C1O UVMRYBDEERADNV-UHFFFAOYSA-N 0.000 claims description 7
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 7
- 229960002217 eugenol Drugs 0.000 claims description 7
- 229920002866 paraformaldehyde Polymers 0.000 claims description 7
- MBYLVOKEDDQJDY-UHFFFAOYSA-N tris(2-aminoethyl)amine Chemical compound NCCN(CCN)CCN MBYLVOKEDDQJDY-UHFFFAOYSA-N 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 4
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 4
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 4
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 229920003009 polyurethane dispersion Polymers 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 3
- 238000009825 accumulation Methods 0.000 abstract description 2
- 230000003373 anti-fouling effect Effects 0.000 abstract description 2
- 239000000428 dust Substances 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 20
- 229910021641 deionized water Inorganic materials 0.000 description 20
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 230000006872 improvement Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 description 6
- ORLPWCUCEDVJNN-UHFFFAOYSA-N sodium;tetradecyl benzenesulfonate Chemical compound [Na].CCCCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 ORLPWCUCEDVJNN-UHFFFAOYSA-N 0.000 description 6
- 238000005034 decoration Methods 0.000 description 5
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000007665 sagging Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- PNGBYKXZVCIZRN-UHFFFAOYSA-M sodium;hexadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCS([O-])(=O)=O PNGBYKXZVCIZRN-UHFFFAOYSA-M 0.000 description 2
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 description 1
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 description 1
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000004264 Petrolatum Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 238000007551 Shore hardness test Methods 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- QLBRROYTTDFLDX-UHFFFAOYSA-N [3-(aminomethyl)cyclohexyl]methanamine Chemical compound NCC1CCCC(CN)C1 QLBRROYTTDFLDX-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 238000002330 electrospray ionisation mass spectrometry Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000011499 joint compound Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- MXXDSLLVYZMTFA-UHFFFAOYSA-N octadecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 MXXDSLLVYZMTFA-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000019271 petrolatum Nutrition 0.000 description 1
- 229940066842 petrolatum Drugs 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229960000776 sodium tetradecyl sulfate Drugs 0.000 description 1
- HEBRGEBJCIKEKX-UHFFFAOYSA-M sodium;2-hexadecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HEBRGEBJCIKEKX-UHFFFAOYSA-M 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- GGHPAKFFUZUEKL-UHFFFAOYSA-M sodium;hexadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCOS([O-])(=O)=O GGHPAKFFUZUEKL-UHFFFAOYSA-M 0.000 description 1
- KBAFDSIZQYCDPK-UHFFFAOYSA-M sodium;octadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCS([O-])(=O)=O KBAFDSIZQYCDPK-UHFFFAOYSA-M 0.000 description 1
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 description 1
- UPUIQOIQVMNQAP-UHFFFAOYSA-M sodium;tetradecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCOS([O-])(=O)=O UPUIQOIQVMNQAP-UHFFFAOYSA-M 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013555 soy sauce Nutrition 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
- C08G59/621—Phenols
- C08G59/623—Aminophenols
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides an environment-friendly joint beautifying composition for ceramic tiles and a preparation method thereof, and belongs to the technical field of joint beautifying agents. Comprises a component A and a component B; the component A comprises aqueous epoxy resin, a defoaming agent, a silane coupling agent, an antioxidant and an initiator; the component B comprises a modified amine curing agent, pearl powder, a diluent, a thixotropic agent, a defoaming agent, triethanolamine and modifier nano powder. The seam beautifying agent composition prepared by the invention is an aqueous composition, has the advantages of environmental protection, less VOC emission, short curing time, low cost, small shrinkage, good anti-fouling performance, good acid and alkali resistance, good toughness, compact and smooth surface, easy cleaning, difficult dust accumulation, good waterproof performance and the like, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of joint beautifying agents, in particular to an environment-friendly joint beautifying composition for ceramic tiles and a preparation method thereof.
Background
The seam-beautifying agent is paid attention to in the last two years and rapidly develops, and is now an essential material in the field of building decoration. On the building decoration, gaps are reserved between the floor wall tiles, a certain amount of filling materials are needed for decoration and beautification, from the past white cement to the later joint filling agent to the current joint filling agent, the product is continuously updated, and the product is greatly improved in terms of beauty, environmental protection and durability. The existing seam beautifying agent has the advantages of antibiosis, mildew resistance, water resistance, no blackening, high glossiness, various colors and the like.
The application field and construction of the joint beautifying agent determine that the joint beautifying agent has to be dried quickly, is convenient for construction and is cleaned in time; the toughness is strong, and the deformation generated by the floor heating expansion and contraction ceramic tile can be borne; the weather resistance is strong, and the light can be subjected to long-time illumination; the hardness is high, and the impact in the long-term use process can be resisted. Based on the above requirements, 1,3-BAC is mainly selected as main alicyclic amine in the industry at present, and IPDA is limited in application because of strong hygroscopicity, and HMDA is limited in application because of slow surface drying time and inconvenient timely cleaning. Too much polyether amine is used in the joint beautifying agent for toughening, so that the curing efficiency is reduced, and the construction efficiency is further reduced; excessive use of the diluent for toughening can lead the hardness and strength of the cured product to be unable to meet the requirements; the physical toughening method can cause the compactness and stability to be greatly influenced after curing.
The bi-component epoxy joint beautifying agent disclosed in Chinese patent CN105802451B has the advantages of no flow, no sagging, convenient construction and the like during construction, but has the defect of poor toughness, and cannot meet the requirement of resisting deformation due to heat expansion and cold contraction in winter in the north.
Chinese patent application CN106634755a discloses a method for preparing epoxy modified HMDA, where the curing agent is used in the field of joint beautifying agent, and can increase the curing speed of HMDA, but the epoxy modified curing agent has a relatively high viscosity, is difficult to mix with thixotropic agent, is difficult to glue, and is very inconvenient for downstream construction.
The Chinese patent application CN106957629A discloses a ceramic tile joint beautifying agent which meets higher requirements on color, hardness and environmental protection, but mainly adjusts the curing speed through DMP-30, and the accelerant is particularly easy to yellow and does not achieve satisfactory effect on long-term durability.
Therefore, the development of the environment-friendly joint composition for ceramic tiles, which has the advantages of bonding fixation, good toughness, cracking resistance, brightness like porcelain (scrubbing resistance), lasting high-efficiency bacteriostasis and mildew resistance (mildew-proof grade (GB/T1741-1989) grade 0), yellowing resistance, waterproof sealing, good construction performance (sagging resistance, wall and ground application, no sagging), green environment protection and meeting the indoor decoration standard (GB 18583-2008), has wide market prospect.
Disclosure of Invention
The invention aims to provide an environment-friendly joint beautifying composition for ceramic tiles and a preparation method thereof, which are aqueous compositions, have the advantages of environmental friendliness, less VOC emission, short curing time, low cost, small shrinkage, good anti-pollution performance, good acid and alkali resistance, good toughness, compact and smooth surface, easy cleaning, difficult ash deposition, good waterproof performance and the like, and have wide application prospects.
The technical scheme of the invention is realized as follows:
the invention provides an environment-friendly joint composition for ceramic tiles, which comprises a component A and a component B; the component A comprises aqueous epoxy resin, a defoaming agent, a silane coupling agent, an antioxidant and an initiator; the component B comprises a modified amine curing agent, pearl powder, a diluent, a thixotropic agent, a defoaming agent, triethanolamine and modifier nano powder;
the modified amine curing agent has a structure as shown in formula I:
the modifier nano powder is modified nano-fold graphene coated silicon oxide microspheres.
As a further improvement of the invention, the component A comprises the following raw materials in parts by weight: 80-100 parts of water-based epoxy resin, 0.3-0.7 part of defoamer, 1-3 parts of silane coupling agent, 0.2-0.3 part of antioxidant and 0.01-0.02 part of initiator; the component B comprises the following raw materials in parts by weight: 30-50 parts of modified amine curing agent, 10-12 parts of pearl powder, 1-3 parts of thixotropic agent, 5-7 parts of diluent, 0.2-0.3 part of defoamer, 3-5 parts of triethanolamine and 10-12 parts of modifier nano powder.
As a further improvement of the invention, the synthesis method of the modified amine curing agent is as follows: and adding the eugenol into the tri (2-amino ethyl) amine under the heating condition, stirring and mixing, then adding the paraformaldehyde, uniformly mixing, heating for reaction, and carrying out vacuum dehydration after the reaction is finished to obtain the product.
As a further improvement of the invention, the mol ratio of eugenol, tri (2-amino ethyl) amine and paraformaldehyde is 1:1.2-1.3:1, the temperature of the heating condition is 80-90 ℃, the stirring and mixing time is 10-20min, the temperature of the heating reaction is 95-105 ℃, and the time is 2-3h.
As a further improvement of the invention, the preparation method of the modifier nanometer powder comprises the following steps:
s1, dissolving alkyl orthosilicate in an organic solvent, adding the organic solvent into an aqueous solution containing a surfactant, emulsifying, adjusting the pH value, stirring for reaction, centrifuging, washing and drying to obtain nano silicon oxide microspheres;
s2, dissolving graphene oxide in water, adding the nano silicon oxide microspheres prepared in the step S1, stirring and mixing uniformly, spray-drying to prepare nano pleated graphene oxide coated silicon oxide microspheres, adding the nano pleated graphene oxide coated silicon oxide microspheres into water, adding hydrazine hydrate and ammonia water, heating and stirring for reaction, centrifuging, washing and drying to prepare nano pleated graphene coated silicon oxide microspheres;
s3, adding the nano-pleated graphene coated silicon oxide microspheres prepared in the step S2 into an ethanol solution, adding a silane coupling agent with double bonds, heating, stirring, reacting, centrifuging, washing and drying to prepare the modifier nano-powder.
As a further improvement of the invention, the alkyl orthosilicate in the step S1 is methyl orthosilicate or ethyl orthosilicate, and the mass ratio of the alkyl orthosilicate to the surfactant is 15-20:1-2; the pH value is adjusted to 9-10, and the stirring reaction time is 5-7h.
As a further improvement of the invention, in the step S2, the mass ratio of the graphene oxide to the nano silicon oxide microspheres is 12-15:20, the mass ratio of the hydrazine hydrate to the ammonia water to the nano-pleated graphene oxide coated silicon oxide microspheres is 3-4:1-2:12-15, the temperature of the heating and stirring reaction is 80-90 ℃ for 1-2 hours, the spray drying condition is that the air inlet temperature is 90-100 ℃, the air outlet temperature is 50-70 ℃, and the evaporation water amount is 1500-2000mL/h.
Preferably, the surfactant is at least one selected from sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium tetradecyl benzene sulfonate, sodium tetradecyl sulfate, sodium hexadecyl sulfonate, sodium hexadecyl benzene sulfonate, sodium hexadecyl sulfate, sodium octadecyl benzene sulfonate, sodium octadecyl sulfonate, and sodium octadecyl sulfate.
Preferably, the organic solvent is at least one selected from petroleum ether, dichloromethane, dichloroethane, toluene, xylene, n-hexane, cyclohexane, ethyl acetate, methyl acetate, butyl acetate.
As a further improvement of the invention, in the step S3, the mass ratio of the nano-pleated graphene coated silicon oxide microspheres to the silane coupling agent with double bonds is 10:1-2, and the silane coupling agent with double bonds is at least one selected from the group consisting of hydroxy methylsilane acrylate and 3-methacryloxypropyl trimethoxysilane; the temperature of the heating and stirring reaction is 60-70 ℃ and the time is 0.5-1h.
As a further improvement of the present invention, the aqueous epoxy resin is at least one selected from CYDW-125, YR-909N, WE401, RD-6607, H4000, WX-700; the diluent is benzyl alcohol; the defoaming agent is at least one selected from polysiloxane defoaming agents, fatty acid amide defoaming agents and phosphate defoaming agents; the silane coupling agent is at least one selected from KH550, KH560, KH570, KH580, KH590, KH602 and KH 792; the thixotropic agent is at least one selected from hydroxyethyl cellulose, polyester urea, methyl acrylate-acrylate copolymer and polyurethane dispersion; the initiator is at least one selected from potassium persulfate, sodium persulfate and ammonium persulfate.
The invention further provides a preparation method of the seam beautifying composition for the environment-friendly ceramic tile, which comprises the following steps of:
(1) Mixing the aqueous epoxy resin, the defoamer, the silane coupling agent, the antioxidant and the initiator in proportion, and mixing for 5-10min at the rotating speed of 1700-2000r/min to prepare a component A;
(2) Mixing pearl powder, thixotropic agent, diluent and defoamer in proportion, mixing for 5-10min at 1700-2000r/min, adding modified amine curing agent, mixing for 3-5min at 1700-2000r/min, adding triethanolamine and modifier nano powder, mixing for 3-5min at 1700-2000r/min to obtain component B;
when the environment-friendly joint beautifying composition for the ceramic tiles is used, the component A and the component B are uniformly mixed according to the ratio of 1:1, construction is carried out, and the environment-friendly joint beautifying composition for the ceramic tiles is cured for 2-4 hours at room temperature.
The invention has the following beneficial effects: the modified amine curing agent prepared by the invention has higher molecular weight, on one hand, the equivalent weight of the modified amine curing agent in reaction with the epoxy resin is increased, so that the ratio of the epoxy resin to the curing agent is increased, and the modified amine curing agent is convenient for batching; on the other hand, the existence of the phenolic hydroxyl can lead the curing reaction of the epoxy resin and the curing agent to be more stable, not to be very violent, strengthen the curing reaction activity and be cured in a wet environment at normal temperature and low temperature (even about 0 ℃); in addition, other groups are introduced into the molecule, so that the crosslinking point of the curing reaction can be effectively reduced, and the brittleness of the cured product and the water absorption of the small molecular amine are reduced. The phenolic aldehyde skeleton structure is introduced into the molecule, so that the heat distortion temperature of the epoxy resin cured product is improved, and the defects of high volatility, high irritation and high toxicity of the lower aliphatic amine are overcome. In addition, due to the existence of benzene rings in the molecules, the curing agent has higher melting point and better crystallinity, and the good thermal stability and excellent mechanical properties of the curing agent are ensured. The modified amine curing agent has the advantages of simple synthetic route, high yield, high reaction purity, good selectivity and milder conditions.
The benzyl alcohol is taken as the diluent, the proper addition amount of the benzyl alcohol can effectively reduce the viscosity of the system, control the reaction heat of the epoxy resin and the curing agent, and adjust the tensile strength and the surface drying time of the joint compound.
In addition, the modified amine curing agent disclosed by the invention can also promote the process of generating a space network structure in a system by coating the silicon oxide with the modified nano-wrinkled graphene, and has a positive effect on playing a thixotropic effect. The double bond of the modified amine curing agent can form a crosslinking system with the double bond of the modified nano-wrinkled graphene coated silicon oxide under the action of an initiator, so that the improvement of mechanical property, corrosion resistance, water resistance, toughness and the like of the system is improved.
According to the invention, the prepared modifier nano powder is modified nano pleated graphene coated silica microspheres, firstly, the nano silica microspheres are prepared by a sol-gel method, then, a layer of pleated graphene oxide is coated on the surface of the nano silica microspheres by a spray drying method, the solvent is rapidly evaporated in the process to cause the volume shrinkage of liquid drops, the pleated graphene microspheres can be obtained by cyclone separation, the nano pleated graphene coated silica is obtained after reduction, the pleated graphene can be obtained, the stacking in a graphene matrix can be reduced by the pleat structure among graphene particles, the aggregation caused by the ordered structure among the graphene is avoided, the uniform dispersion is realized, and the excellent performance of the graphene is fully exerted; after the surface is modified by a silane coupling agent with double bonds, the surface of the prepared product is not only provided with a hydrophobic and oleophobic corrugated graphite layer, but also provided with double bond groups, and the product can be crosslinked with a modified amine curing agent to form a network structure, so that the improvement of mechanical property, corrosion resistance, water resistance, toughness and the like of the system is further improved. In the invention, when the usage amount of the modifier nano powder is more, uneven dispersion can reduce the glossiness of a cured product, and the silicon hydroxyl groups on the surface of the modifier nano powder can also react with epoxy groups, so that the reaction time of the curing agent and the epoxy resin is shortened, and the mechanical property of the cured product is improved.
The seam beautifying agent composition prepared by the invention is an aqueous composition, has the advantages of environmental protection, less VOC emission, short curing time, low cost, small shrinkage, good anti-fouling performance, good acid and alkali resistance, good toughness, compact and smooth surface, easy cleaning, difficult dust accumulation, good waterproof performance and the like, and has wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is an SEM image of the modifier nanometer powder prepared in preparation example 4 of the invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Preparation example 1 Synthesis of modified amine curing agent
The synthetic route is as follows:
the method comprises the following steps: heating 0.1mol of eugenol to 80 ℃, adding 0.12mol of tri (2-aminoethyl) amine, stirring and mixing for 10min, then adding a 36wt% paraformaldehyde aqueous solution containing 0.1mol, uniformly mixing, heating to 95 ℃, reacting for 2h, and vacuum dehydrating after the reaction is finished to obtain a product, wherein the calculated value of ESI-MS is as follows: c (C) 17 H 31 N 4 O 2 (m+h) +323.24, found: 323.2, the yield thereof was found to be 92.6%.
Nuclear magnetic results: 1 H NMR(300MHz，CDCl 3 )δ6.21-6.30(m，3H)，4.92-5.0(m，3H)，3.82(d，2H)，3.72(s，3H)，3.22(d，2H)，2.75(m，4H)，2.62-2.65(m，6H)，2.48(t，2H)，2.0(br，5H)。
preparation example 2 Synthesis of modified amine curing agent
The method comprises the following steps: heating 0.1mol of eugenol to 90 ℃, adding 0.13mol of tri (2-aminoethyl) amine, stirring and mixing for 20min, then adding a 36wt% paraformaldehyde aqueous solution containing 0.1mol, uniformly mixing, heating to 105 ℃, reacting for 3h, and vacuum dehydrating after the reaction is finished to obtain the product with the yield of 93.2%.
Preparation example 3 Synthesis of modified amine curing agent
The method comprises the following steps: heating 0.1mol of eugenol to 85 ℃, adding 0.125mol of tri (2-aminoethyl) amine, stirring and mixing for 15min, then adding a 36wt% paraformaldehyde aqueous solution containing 0.1mol, uniformly mixing, heating to 100 ℃, reacting for 2.5h, and vacuum dehydrating after the reaction is finished to obtain a product with the yield of 93.0%.
Preparation example 4 preparation of modifier nanopowder
The method comprises the following steps:
s1, dissolving 15 parts by weight of methyl orthosilicate in 50 parts by weight of ethyl acetate, adding 100 parts by weight of aqueous solution containing 1 part by weight of sodium dodecyl benzene sulfonate, emulsifying for 20min at 12000r/min, adjusting the pH value to 9, stirring and reacting for 5h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to obtain nano silicon oxide microspheres;
s2, dissolving 12 parts by weight of graphene oxide in 100 parts by weight of water, adding 20 parts by weight of the nano silicon oxide microspheres prepared in the step S1, stirring and mixing for 20min, spray-drying to prepare nano pleated graphene oxide coated silicon oxide microspheres, adding 12 parts by weight of nano pleated graphene oxide coated silicon oxide microspheres into 100 parts by weight of water, adding 3 parts by weight of hydrazine hydrate and 1 part by weight of 25wt% ammonia water, heating to 80 ℃, stirring and reacting for 1h, centrifuging for 15min 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to prepare nano pleated graphene coated silicon oxide microspheres;
the spray drying condition is that the air inlet temperature is 90 ℃, the air outlet temperature is 50 ℃ and the evaporation water quantity is 1500mL/h;
s3, adding 10 parts by weight of the nano-pleated graphene coated silicon oxide microspheres prepared in the step S2 into 100 parts by weight of 70wt% ethanol solution, adding 1 part by weight of 3-methacryloxypropyl trimethoxysilane, heating to 60 ℃, stirring and reacting for 0.5h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to prepare the modifier nano-powder. Fig. 1 is an SEM image of the resulting modifier nano-powder, which is shown to have a surface-corrugated structure.
Preparation example 5 preparation of modifier nanopowder
The method comprises the following steps:
s1, dissolving 20 parts by weight of ethyl orthosilicate in 50 parts by weight of petroleum ether, adding 100 parts by weight of aqueous solution containing 2 parts by weight of sodium hexadecyl sulfonate, emulsifying for 20min at 12000r/min, adjusting the pH value to 10, stirring for reaction for 7h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to obtain nano silicon oxide microspheres;
s2, dissolving 15 parts by weight of graphene oxide in 100 parts by weight of water, adding 20 parts by weight of the nano silicon oxide microspheres prepared in the step S1, stirring and mixing for 20min, spray-drying to prepare nano pleated graphene oxide coated silicon oxide microspheres, adding 15 parts by weight of nano pleated graphene oxide coated silicon oxide microspheres into 100 parts by weight of water, adding 4 parts by weight of hydrazine hydrate and 2 parts by weight of 25wt% ammonia water, heating to 90 ℃, stirring and reacting for 2h, centrifuging for 15min 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to prepare nano pleated graphene coated silicon oxide microspheres;
the spray drying condition is that the air inlet temperature is 100 ℃, the air outlet temperature is 70 ℃ and the evaporation water quantity is 2000mL/h;
s3, adding 10 parts by weight of the nano-pleated graphene coated silicon oxide microspheres prepared in the step S2 into 100 parts by weight of 70wt% ethanol solution, adding 2 parts by weight of 3-methacryloxypropyl trimethoxysilane, heating to 70 ℃, stirring and reacting for 1h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to prepare the modifier nano-powder.
Preparation example 6 preparation of modifier nanopowder
The method comprises the following steps:
s1, dissolving 17 parts by weight of ethyl orthosilicate in 50 parts by weight of n-hexane, adding 100 parts by weight of an aqueous solution containing 1.5 parts by weight of sodium tetradecyl benzenesulfonate, emulsifying for 20min at 12000r/min, adjusting the pH value to 9.5, stirring for reaction for 6h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to obtain nano silicon oxide microspheres;
s2, dissolving 13.5 parts by weight of graphene oxide in 100 parts by weight of water, adding 20 parts by weight of the nano silicon oxide microspheres prepared in the step S1, stirring and mixing for 20min, spray-drying to prepare nano pleated graphene oxide coated silicon oxide microspheres, adding 13.5 parts by weight of nano pleated graphene oxide coated silicon oxide microspheres into 100 parts by weight of water, adding 3.5 parts by weight of hydrazine hydrate and 1.5 parts by weight of 25wt% ammonia water, heating to 85 ℃, stirring and reacting for 1.5h, centrifuging for 15min 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to prepare nano pleated graphene coated silicon oxide microspheres;
the spray drying condition is that the air inlet temperature is 95 ℃, the air outlet temperature is 60 ℃ and the evaporation water quantity is 1700mL/h;
s3, adding 10 parts by weight of the nano-pleated graphene coated silicon oxide microspheres prepared in the step S2 into 100 parts by weight of 70wt% ethanol solution, adding 1.5 parts by weight of 3-methacryloxypropyl trimethoxysilane, heating to 65 ℃, stirring and reacting for 1h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to prepare the modifier nano-powder.
Comparative preparation example 1
In comparison with preparation example 6, the difference is that step S1 is not performed.
The method comprises the following steps:
s1, dissolving 33.5 parts by weight of graphene oxide in 100 parts by weight of water, spray-drying to obtain nano-pleated graphene oxide microspheres, adding 13.5 parts by weight of nano-pleated graphene oxide microspheres into 100 parts by weight of water, adding 3.5 parts by weight of hydrazine hydrate and 1.5 parts by weight of 25wt% ammonia water, heating to 85 ℃, stirring for reacting for 1.5 hours, centrifuging for 15 minutes at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1 hour to obtain nano-pleated graphene coated microspheres;
the spray drying condition is that the air inlet temperature is 95 ℃, the air outlet temperature is 60 ℃ and the evaporation water quantity is 1700mL/h;
s2, adding 10 parts by weight of the nano-wrinkled graphene microspheres prepared in the step S2 into 100 parts by weight of 70wt% ethanol solution, adding 1.5 parts by weight of 3-methacryloxypropyl trimethoxysilane, heating to 65 ℃, stirring and reacting for 1h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying for 1h at 105 ℃ to prepare the modifier nano-powder.
Comparative preparation example 2
In comparison with preparation example 6, the difference is that spray drying is not performed in step S2.
The method comprises the following steps:
s1, dissolving 17 parts by weight of ethyl orthosilicate in 50 parts by weight of n-hexane, adding 100 parts by weight of an aqueous solution containing 1.5 parts by weight of sodium tetradecyl benzenesulfonate, emulsifying for 20min at 12000r/min, adjusting the pH value to 9.5, stirring for reaction for 6h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to obtain nano silicon oxide microspheres;
s2, dissolving 13.5 parts by weight of graphene oxide in 100 parts by weight of water, adding 20 parts by weight of the nano silicon oxide microspheres prepared in the step S1, stirring and mixing for 20min, drying to prepare nano graphene oxide coated silicon oxide microspheres, adding 13.5 parts by weight of nano graphene oxide coated silicon oxide microspheres into 100 parts by weight of water, adding 3.5 parts by weight of hydrazine hydrate and 1.5 parts by weight of 25wt% ammonia water, heating to 85 ℃, stirring and reacting for 1.5h, centrifuging for 15min 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to prepare nano graphene coated silicon oxide microspheres;
the spray drying condition is that the air inlet temperature is 95 ℃, the air outlet temperature is 60 ℃ and the evaporation water quantity is 1700mL/h;
s3, adding 10 parts by weight of the nano graphene coated silica microspheres prepared in the step S2 into 100 parts by weight of 70wt% ethanol solution, adding 1.5 parts by weight of 3-methacryloxypropyl trimethoxysilane, heating to 65 ℃, stirring and reacting for 1h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to prepare the modifier nano powder.
Comparative preparation example 3
In comparison with preparation example 6, the difference is that no reduction is performed in step S2.
The method comprises the following steps:
s1, dissolving 17 parts by weight of ethyl orthosilicate in 50 parts by weight of n-hexane, adding 100 parts by weight of an aqueous solution containing 1.5 parts by weight of sodium tetradecyl benzenesulfonate, emulsifying for 20min at 12000r/min, adjusting the pH value to 9.5, stirring for reaction for 6h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to obtain nano silicon oxide microspheres;
s2, dissolving 13.5 parts by weight of graphene oxide in 100 parts by weight of water, adding 20 parts by weight of the nano silicon oxide microspheres prepared in the step S1, stirring and mixing for 20min, and spray-drying to prepare nano-pleated graphene oxide coated silicon oxide microspheres;
the spray drying condition is that the air inlet temperature is 95 ℃, the air outlet temperature is 60 ℃ and the evaporation water quantity is 1700mL/h;
s3, adding 10 parts by weight of the nano-pleated graphene oxide coated silica microspheres prepared in the step S2 into 100 parts by weight of 70wt% ethanol solution, adding 1.5 parts by weight of 3-methacryloxypropyl trimethoxy silane, heating to 65 ℃, stirring and reacting for 1h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying for 1h at 105 ℃ to prepare the modifier nano-powder.
Comparative preparation example 4
In comparison with preparation example 6, the difference is that step S2 is not performed.
The method comprises the following steps:
s1, dissolving 17 parts by weight of ethyl orthosilicate in 50 parts by weight of n-hexane, adding 100 parts by weight of an aqueous solution containing 1.5 parts by weight of sodium tetradecyl benzenesulfonate, emulsifying for 20min at 12000r/min, adjusting the pH value to 9.5, stirring for reaction for 6h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to obtain nano silicon oxide microspheres;
s2, adding 10 parts by weight of the nano silicon oxide microspheres prepared in the step S1 into 100 parts by weight of 70wt% ethanol solution, adding 1.5 parts by weight of 3-methacryloxypropyl trimethoxy silane, heating to 65 ℃, stirring and reacting for 1h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying for 1h at 105 ℃ to prepare the modifier nano powder.
Comparative preparation example 5
In comparison with preparation example 6, the difference is that step S3 is not performed.
The method comprises the following steps:
s1, dissolving 17 parts by weight of ethyl orthosilicate in 50 parts by weight of n-hexane, adding 100 parts by weight of an aqueous solution containing 1.5 parts by weight of sodium tetradecyl benzenesulfonate, emulsifying for 20min at 12000r/min, adjusting the pH value to 9.5, stirring for reaction for 6h, centrifuging for 15min at 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to obtain nano silicon oxide microspheres;
s2, dissolving 13.5 parts by weight of graphene oxide in 100 parts by weight of water, adding 20 parts by weight of the nano silicon oxide microspheres prepared in the step S1, stirring and mixing for 20min, spray-drying to prepare nano pleated graphene oxide coated silicon oxide microspheres, adding 13.5 parts by weight of nano pleated graphene oxide coated silicon oxide microspheres into 100 parts by weight of water, adding 3.5 parts by weight of hydrazine hydrate and 1.5 parts by weight of 25wt% ammonia water, heating to 85 ℃, stirring and reacting for 1.5h, centrifuging for 15min 3000r/min, washing with deionized water, and drying at 105 ℃ for 1h to prepare nano pleated graphene coated silicon oxide microspheres, namely modifier nano powder;
the spray drying condition is that the air inlet temperature is 95 ℃, the air outlet temperature is 60 ℃ and the evaporation water quantity is 1700mL/h.
Example 1
The embodiment provides a seam beautifying composition for environment-friendly ceramic tiles.
The composite material comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 400080 parts of aqueous epoxy resin H, 0.3 part of defoamer, 5601 parts of silane coupling agent KH, 0.2 part of antioxidant hydroxybenzoate and 0.01 part of potassium persulfate; the component B comprises the following raw materials in parts by weight: 30 parts of modified amine curing agent prepared in preparation example 1, 10 parts of pearl powder, 1 part of polyester urea, 5 parts of benzyl alcohol, 0240.2 parts of defoamer BYK-0240.2 parts, 3 parts of triethanolamine and 10 parts of modifier nano powder prepared in preparation example 4.
The preparation method comprises the following steps:
(1) Mixing aqueous epoxy resin H4000, a defoaming agent, a silane coupling agent KH560, antioxidant hydroxybenzoate and potassium persulfate according to a proportion, and mixing for 5min at a rotation speed of 1700r/min to obtain a component A;
(2) Mixing pearl powder, polyester urea, benzyl alcohol and a defoaming agent BYK-024 in proportion, mixing for 5min at 1700r/min, adding a modified amine curing agent, mixing for 3min at 1700r/min, adding triethanolamine and a modifying agent nano powder, and mixing for 3min at 1700r/min to obtain a component B;
when the environment-friendly joint beautifying composition for the ceramic tiles is used, the component A and the component B are uniformly mixed according to the ratio of 1:1, construction is carried out, and the environment-friendly joint beautifying composition for the ceramic tiles is cured for 2 hours at room temperature.
Example 2
The embodiment provides a seam beautifying composition for environment-friendly ceramic tiles.
The composite material comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: waterborne epoxy resin RD-6607100 parts, defoamer 0.7 parts, silane coupling agent KH5803 parts, antioxidant hydroxybenzoate 0.3 parts and sodium persulfate 0.02 parts; the component B comprises the following raw materials in parts by weight: 50 parts of modified amine curing agent prepared in preparation example 2, 12 parts of pearl powder, 3 parts of methyl acrylate-acrylic ester copolymer, 7 parts of benzyl alcohol, 7100.3 parts of defoamer AG-7100.3 parts of triethanolamine and 12 parts of modifier nano powder prepared in preparation example 5.
The preparation method comprises the following steps:
(1) Mixing the aqueous epoxy resin RD-6607, the defoamer, the silane coupling agent KH580, the antioxidant hydroxybenzoate and the sodium persulfate according to a proportion, and mixing for 10min at a rotating speed of 2000r/min to obtain a component A;
(2) Mixing pearl powder, methyl acrylate-acrylic ester copolymer, benzyl alcohol and defoamer AG-710 in proportion, mixing for 10min at a rotation speed of 2000r/min, adding modified amine curing agent, mixing for 5min at a rotation speed of 2000r/min, adding triethanolamine and modifier nano powder, and mixing for 5min at a rotation speed of 2000r/min to obtain a component B;
when the environment-friendly joint beautifying composition for the ceramic tiles is used, the component A and the component B are uniformly mixed according to the ratio of 1:1, construction is carried out, and the environment-friendly joint beautifying composition for the ceramic tiles is cured for 4 hours at room temperature.
Example 3
The embodiment provides a seam beautifying composition for environment-friendly ceramic tiles.
The composite material comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: water-based epoxy resin WX-70090 parts, defoaming agent 0.5 parts, silane coupling agent KH5902 parts, antioxidant hydroxybenzoate 0.25 parts and ammonium persulfate 0.015 parts; the component B comprises the following raw materials in parts by weight: 40 parts of modified amine curing agent prepared in preparation example 3, 11 parts of pearl powder, 2 parts of hydroxyethyl cellulose, 6 parts of benzyl alcohol, 900.25 parts of defoamer KM, 4 parts of triethanolamine and 11 parts of modifier nano powder prepared in preparation example 6.
The preparation method comprises the following steps:
(1) Mixing water-based epoxy resin WX-700, a defoaming agent, a silane coupling agent KH590, antioxidant hydroxybenzoate and ammonium persulfate according to a certain proportion, and mixing for 7min at 1850r/min to obtain a component A;
(2) Mixing pearl powder, hydroxyethyl cellulose, benzyl alcohol and a defoaming agent KM-90 in proportion, mixing for 7min at 1850r/min, adding a modified amine curing agent, mixing for 4min at 1850r/min, adding triethanolamine and a modifier nano powder, and mixing for 4min at 1850r/min to obtain a component B;
when the environment-friendly joint beautifying composition for the ceramic tiles is used, the component A and the component B are uniformly mixed according to the ratio of 1:1, construction is carried out, and the environment-friendly joint beautifying composition for the ceramic tiles is cured for 3 hours at room temperature.
Comparative examples 1 to 5
The difference compared to example 3 is that modifier nanopowders were prepared from comparative preparation examples 1-5, respectively.
Comparative example 6
The difference compared to example 3 is that the modified amine curing agent is replaced by triethylenediamine.
Comparative example 7
The difference compared to example 3 is that the modified amine curing agent is replaced by a commercially available curing agent (methyl ethyl ketone peroxide, wan Qing chemical technology Co., ltd.).
Test example 1
The environmental-friendly joint composition for ceramic tiles prepared in examples 1 to 3 and comparative examples 1 to 7 of the present invention were subjected to comprehensive performance experiments, and the results are shown in tables 1 and 2.
Drying time: according to GB/T1728-1979, wherein the surface dry is tested according to the method B and the real dry is tested according to the rule A; shore hardness: measuring according to a D-type standard of a GB/T2411-2008 plastic Shore hardness test method; adhesion force: the test is carried out according to the specification of GB/T9286, the spacing between the frames is 2mm, and no adhesive tape is used; looking at sag: the test was carried out according to the method specified in GB/T9264-2012. The tooth distance of the coater is 3mm, and the tooth height is 3mm; water resistance (168 h): the test was carried out according to the A-rule of GB/T1733-1993; bond strength: the measurement is carried out according to JC/T547-2017 standard; and (3) washing resistance: the measurement is carried out according to the GB/T9266-1988 standard; stain resistance: the stain resistance test method is used for measuring the stain resistance of the GB/T9780-2013 interior wall coating. The test medium does not include: alcohol-soluble melanin, petrolatum carbon black mixture; the soy sauce is added. Abrasion resistance (750 g/500 r): the measurement was carried out according to GB/T3810.6-2006.
TABLE 1
TABLE 2
As can be seen from the above table, the environmentally friendly joint composition for ceramic tiles prepared in examples 1 to 3 of the present invention has good comprehensive properties.
Test example 2 environmental protection test
The environmental-friendly joint composition for ceramic tiles prepared in examples 1-3 and comparative examples 1-7 according to the invention was tested for the content of harmful substances in the product according to GB18583-2008 "limit of the amount of harmful substances in interior decoration Material Adhesives", and the results are shown in Table 3.
TABLE 3 Table 3
As can be seen from the above table, the environmentally-friendly joint composition for ceramic tiles prepared in examples 1-3 of the invention has good environmental protection performance.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. The seam beautifying composition for the environment-friendly ceramic tile is characterized by comprising a component A and a component B; the component A comprises aqueous epoxy resin, a defoaming agent, a silane coupling agent, an antioxidant and an initiator; the component B comprises a modified amine curing agent, pearl powder, a diluent, a thixotropic agent, a defoaming agent, triethanolamine and modifier nano powder;
the modified amine curing agent has a structure as shown in formula I:
the modifier nano powder is modified nano-fold graphene coated silicon oxide microspheres.
2. The environmentally friendly joint composition for ceramic tiles according to claim 1, wherein the component a comprises the following raw materials in parts by weight: 80-100 parts of water-based epoxy resin, 0.3-0.7 part of defoamer, 1-3 parts of silane coupling agent, 0.2-0.3 part of antioxidant and 0.01-0.02 part of initiator; the component B comprises the following raw materials in parts by weight: 30-50 parts of modified amine curing agent, 10-12 parts of pearl powder, 1-3 parts of thixotropic agent, 5-7 parts of diluent, 0.2-0.3 part of defoamer, 3-5 parts of triethanolamine and 10-12 parts of modifier nano powder.
3. The environmentally friendly tile seam composition according to claim 1 wherein the modified amine curing agent is synthesized by the following method: and adding the eugenol into the tri (2-amino ethyl) amine under the heating condition, stirring and mixing, then adding the paraformaldehyde, uniformly mixing, heating for reaction, and carrying out vacuum dehydration after the reaction is finished to obtain the product.
4. The composition for environmental protection according to claim 3, wherein the molar ratio of eugenol, tri (2-aminoethyl) amine and paraformaldehyde is 1:1.2-1.3:1, the temperature of the heating condition is 80-90 ℃, the stirring and mixing time is 10-20min, the temperature of the heating reaction is 95-105 ℃ and the time is 2-3h.
5. The environmentally friendly joint composition for ceramic tiles according to claim 1, wherein the modifier nano-powder is prepared by the following method:
s1, dissolving alkyl orthosilicate in an organic solvent, adding the organic solvent into an aqueous solution containing a surfactant, emulsifying, adjusting the pH value, stirring for reaction, centrifuging, washing and drying to obtain nano silicon oxide microspheres;
s2, dissolving graphene oxide in water, adding the nano silicon oxide microspheres prepared in the step S1, stirring and mixing uniformly, spray-drying to prepare nano pleated graphene oxide coated silicon oxide microspheres, adding the nano pleated graphene oxide coated silicon oxide microspheres into water, adding hydrazine hydrate and ammonia water, heating and stirring for reaction, centrifuging, washing and drying to prepare nano pleated graphene coated silicon oxide microspheres;
s3, adding the nano-pleated graphene coated silicon oxide microspheres prepared in the step S2 into an ethanol solution, adding a silane coupling agent with double bonds, heating, stirring, reacting, centrifuging, washing and drying to prepare the modifier nano-powder.
6. The environmentally friendly joint composition for ceramic tiles according to claim 5, wherein the alkyl orthosilicate in the step S1 is methyl orthosilicate or ethyl orthosilicate, and the mass ratio of the alkyl orthosilicate to the surfactant is 15-20:1-2; the pH value is adjusted to 9-10, and the stirring reaction time is 5-7h.
7. The environment-friendly joint composition for ceramic tiles of claim 5, wherein in the step S2, the mass ratio of graphene oxide to nano silicon oxide microspheres is 12-15:20, the mass ratio of hydrazine hydrate to ammonia water to nano-fold graphene oxide coated silicon oxide microspheres is 3-4:1-2:12-15, the temperature of heating and stirring reaction is 80-90 ℃ for 1-2h, the condition of spray drying is that the air inlet temperature is 90-100 ℃, the air outlet temperature is 50-70 ℃, and the evaporation water amount is 1500-2000mL/h.
8. The environmentally friendly joint composition for ceramic tiles according to claim 5, wherein in the step S3, the mass ratio of the nano-wrinkled graphene coated silica microspheres to the silane coupling agent with double bonds is 10:1-2, and the silane coupling agent with double bonds is at least one selected from the group consisting of hydroxymethyl-silane acrylate and 3-methacryloxypropyl trimethoxysilane; the temperature of the heating and stirring reaction is 60-70 ℃ and the time is 0.5-1h.
9. The environmentally friendly joint composition for ceramic tiles according to claim 1, wherein the aqueous epoxy resin is at least one selected from CYDW-125, YR-909N, WE401, RD-6607, H4000, WX-700; the diluent is benzyl alcohol; the defoaming agent is at least one selected from polysiloxane defoaming agents, fatty acid amide defoaming agents and phosphate defoaming agents; the silane coupling agent is at least one selected from KH550, KH560, KH570, KH580, KH590, KH602 and KH 792; the thixotropic agent is at least one selected from hydroxyethyl cellulose, polyester urea, methyl acrylate-acrylate copolymer and polyurethane dispersion; the initiator is at least one selected from potassium persulfate, sodium persulfate and ammonium persulfate.
10. A method of preparing the decorative joint composition for environmental protection tiles according to any one of claims 1 to 9, comprising the steps of:
(1) Mixing the aqueous epoxy resin, the defoamer, the silane coupling agent, the antioxidant and the initiator in proportion, and mixing for 5-10min at the rotating speed of 1700-2000r/min to prepare a component A;
(2) Mixing pearl powder, thixotropic agent, diluent and defoamer in proportion, mixing for 5-10min at 1700-2000r/min, adding modified amine curing agent, mixing for 3-5min at 1700-2000r/min, adding triethanolamine and modifier nano powder, mixing for 3-5min at 1700-2000r/min to obtain component B;
when the environment-friendly joint beautifying composition for the ceramic tiles is used, the component A and the component B are uniformly mixed according to the ratio of 1:1, construction is carried out, and the environment-friendly joint beautifying composition for the ceramic tiles is cured for 2-4 hours at room temperature.
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| US20200040196A1 (en) * | 2017-03-24 | 2020-02-06 | 3M Innovative Properties Company | Aqueous primer composition and related methods |
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| CN113698846A (en) * | 2021-09-07 | 2021-11-26 | 江苏冠军科技集团股份有限公司 | Hyperbranched epoxy zinc-rich coating and preparation method thereof |
| CN116904152A (en) * | 2023-05-08 | 2023-10-20 | 广东靓砂建材科技有限公司 | Environment-friendly joint beautifying composition for ceramic tiles and preparation method thereof |
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| US20200040196A1 (en) * | 2017-03-24 | 2020-02-06 | 3M Innovative Properties Company | Aqueous primer composition and related methods |
| CN109486455A (en) * | 2017-09-12 | 2019-03-19 | 上海域金澜优电子商务有限公司 | A kind of novel nano fungus and mildew resistance water-base epoxy joint trimming agent |
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